Extraction apparatus



July 27,1926.

l R. P. SOULE EXTRACTION APPARATUS Filed June Il .l

Patented July 27, 1926. 'i

UNITED STATES ROLAND P.

PATENT orifice..l

SOULE, OF NEW YORK, 4N. Y., ASSIGNOR T0 COMBUSTIO UTILITIES COB- ,POBATIONQ OIF NEW YORK, N. Y., .A CORPORATION QFYMAIN'E.

Exrna'c'rron APPARATUS.

Application and time 11,

This invention relates to an extraction apparatus, and particularly to'an apparatus in which the soluble components of a liquid mixture Vcan be continuously extracted under pressure.

-Water, for example, may be such a solvent.

oil p Thus, the phenols in a phenol-bearin such as a coal-tar distillate are only slightl soluble in water at room temperature 20 0.). The are more soluble in boiling water (100 C. but still insuiiiciently solubleto be economically extracted. They are extremely soluble in water above 200 C., however, and can be extracted successfully at such temperatures.

The 'difficulties involved in the 4development of en ,apparatus in which this principlecan be utilized etliciently are two-fold, and are suiciently great to have prevented its extensivecommercial application before the present time. In the yfirst place, the principal operations of the extraction proc ess, such as agitation, settling, and the sepa'- ration of layers, must `all be erformed under pressures suiiiciently hig to maintain the' solvent in its liquid phase at thev elevated temperatures in question In the second place, considerations of reconomy y in both plant investment and o rating expenditures require in addition t atthese various, operations of the process be conducted continuously and without interru tion. In

intermittent operation the productmn capacity of the extraction apparatus is 'diminished in proportion to the time lost in heating l its contents to the desired temperature.

Moreover, the fuel requirements are excessive to the extent that heat is lost from the hot products ofv extraction.` A high t'l'ier-l maleconomy of operation can be obtamed 1924. Serial'No. 719,281.

only when such heat is transferred tothe incoming cold charge. This transfer can be accomplished efficiently only when the liquid mixture and its lsolvent are introduced continuously and when the products of extraction are Withdrawn continuously. l,

One object of the present invention is to provide an apparatus in which a liquid Lolixture can be subjected under pressure to the various operations of extraction, such as agitation, settling, vand the separation of paratus.

Another object of the invention is to pro vide an ap aratus by means of which Water can b e used) as the solvent in the commercial extraction of phenols from phenol-bearing oils, such as coal-tar distillates and similar liquid mixtures.

Other objects and features of the invention will appear in. the `following description and in the claims.

A 'schematicillustration of a preferred l arrangement of the apparatus forming the subject matter of the present invention .is given in the accompanying drawinggshowing the application of the invention to the aqueous extraction of phenols from a phenol-bearing oil;

In the drawing Fig. 1 is a view, partly in elevation and partly in section, which shows the extraction autoclave" and its arrangement with auxiliary pumping, separating, mixing and eheating units to form a closed circuit or the solvent, and

Fig. 2 is a cross sectional view of the interior of the autoclave taken on the line` 2 2 of Fig. 1.

The ap aratus constituting the preferredform of t e invention consists essentially of y ssj an autoclave or pressure vessel divided into a mixing or extraction chamber and a settling chamber, and connected by supply pipes and discharge pipes to auxiliary pumping, separating, mixing and heat ex'- changing or preheating'units. The'autoclave is preferably supported at an angle to the horizontal. Themxing chamber is preferably enclosed within the combustion zone of a heating furnace, so thatV the heat necessary to obtain the desired temperature can be supplied to the material while it is being extracted with the solvent. In the operation of the apparatus vthe liquid to be extracted, mixed' with the solvent in a fixed proportion, is charged into the mixing chamber through a spray nozzle in such a way as to create a continuous circulation and agitation of the charge throughout the per'iod of its extraction therein. Heat is ap' plied directly to .the bottom and side walls of the mixing chamber and thecharge in both chambers is maintained at a temperature above the boiling point of the solvent and under suicient pressure to prevent its ebullition. As a result both of the increased solubility and reduced viscosity of the charge at this high temperature and of the thorough agitation induced by the method of char ing, extraction can be made to take lace a ost as ra idly as fresh liquid is introduced. This resh liquidv is continuously charged into the mixing chamber and a loose emulsion of the extract with the insoluble components, of the liquid is continuously displacedover a baiile plate or Weir into a settling chamber. In this settling chamber the emulsion is maintained, in a quiescent state at the same pressure and substantially the'same temperature as exist in the mixing chamber. Under these conditions the emulsion rapidly separates into layers of its component parts, i. e., the solution of the soluble components in the solvent and the insoluble components. These layers settle to the bottom or rise to the top of the chamber, accordingto their relative specific gravities, and are continuously and separately discharged from the settling chamber. The charging pump and valves in the discharge p1 es', moreover, are so regulated that the llquids ate charged into the autoclave and discharged therefrom at a rate not in excess of that at which the extraction and separation of layers is completed therein.l The hot eiiiuents discharged from the settling chamber pass through auxiliary preheatmg equipmentr in heat interchanglng relatlonship with the mixture of the solyent and the liquid to be extracted on their way to tbe mixing chamber. By this vmeansheat carried from 'the autoclave by the departing liquids is utilized in preheating the entering liquids', and the thermal disclosed in this connection forms the subp ject of a separate invention, ferwhich a patent application has vbe-entiled May 3l, 1924, Serial No.'716,899, by Stephen P. Burke.

so f

The liquid to be extracted in this particu Y lar application of t-he invention is described as a phenol-bearing oil ores fresh oil. This oil is pumped or otherwise introduced into a tank 10. From the tank 10 the fresh oil is led through a pipe 12 to a mixing tank 14, wherein it is mixed with Water introduced through a pipe 16,-water in this case serv-l ing as a solvent or extraction agent- The agitator and most of the other auxiliary equipment hereinafter described may be of any standard type. The vagitator illustrated in the drawings is shown equipped with paddles driven by a power shaft through gears 18. After being thoroughly.

mixed in the agitator the mixture of fresh oil and Water is passed through a pipe 20. carrying a strainer 21, into the. cylinder of a circulating pump 22, which raises it by a pipe line 24 to a constant gravity supply tank 26.V Any overiow from the supply tank 26 is returned to the agitator by a pipe 28 and to provide against overiiow from the agitator 14 a drawoif pipe 30 is so connected vthat any excess oil and water overflows and is conducted to a water-oil decanter 32, where the water and oil separate and can be run oii' to respective storage tanks34 and 36. From the constant-feed or supply tank 26 the properly proportioned mixture of oil and Water is passed through a pipe 38 into the bottom of a preheater or heat exchanger 40, wherein it is vgradually heated as it rises toward an outlet pipe/42 by heat transfer with previously heated liquids passing downwardly through a coil 44. From the preheater 40 the mixture lof oil and W'ater passes through theI ipe 42 into the bottom of another heat. exc anger or preheater r46. similar in design 'to preheater 40, wherein the mixture is further heated by heat trans; fer with other hot liquids vpassing through coil 48. From thepreheater 46 thevmixture of oil and water passes through a pipe 50 and a strainer 52 into the cylinder of a high pressure feed pum 54 and is forced by this pump through a pipe 55 and a control valve 56 and check valve 57 into an antoclave 58.

If further preheating of the charging mixture of oil and water is found necessary it may be accomplished by passing it through other heat interchanging apparatus, preferably connected in the line at some point b etween the charging pump 54 and the check valve 57. Heat 'necessary fortheadditional preheating can be supplied by the hot gaseous products of combustion from the heating furnace shown, or in any other feasible manner. v

The autoclave 58 consists essentially of a cylindrical pressure vessel which is supported at an angle with the horizontal and has' its u perendenclosed within a furnace combustlon chamber 60. The lower exposed end of the autoclave, which lies outside of.A the furnace setting is preferably protected by a coating of heat insulating material to prevent loss of heat by radiation, The severalcharging pipes 42, 50 and 55, the cylinders of the charging pump 54, and the preheaters 40 and 46 may' also be wrapped to advantage with similar heat insulatlng material. `The length of the autoclave cylinder and the angle at' which it is' supported are both determined by the rate at which material can be passed through the autoclave, which in turn depends on the rate at which the extraction is completed, or at which the aqueous solution of the phenols subsequently separates by gravity 'action from the insoluble residual oil. y

The inside of the autoclave isdivide-d by a vertical weir or baiile plate 61 into two sections or chambers. --The smaller sectionv is' in the upper end of the autoclave and isentirely enclosed by the furnace combustion chamber, and it is into this section .that the feed pi e 55 discharges. -To the pipe 55 is attached a spray nozzle 62 which is provided with jet openings through which the mixture ofIv oil and water is vdirected with high velocity against the hot bottom of the auto; clave. By this means the mixture ef hot oil and water is introduced below the surface of the charge and is directed by abafile plate 63, as shown in Fig.'2, to pass upwardsl alng the hot walls of the, u per or mixing chamber. Gas or other fuel 1s burned in the combustion chamber of furnace 60, and the v oil-water mixture charged through nozzle 62 to imping'e in numerous small jets travelingv at high velocity against the hot bottom, that A portion of the body of the charge in the upper or mixing chamber of the autoclave is maintained atthe deslred temperature an is kept in a state of continuous circulation tion of the oil and water in the mixing cham- V berare displaced by the incoming mixture they' flow continuouslyy over .the topv of j the weir 61 into the larger settling chamber 65, cpmprising'the .lower section of the autoc ave.

per or mixing chamber and the lower or settling chamber, and the pressure within this vapor space is maintained high enough to prevent boiling of the water and oil ciontained in the autoclave. A pressure gauge' 66 and a safety valve 68 are attached to the The vapor space 64 overlies both the up-v A thermostatically v the autoclave can be automatically regulated. The pressures within the autoclave can bev regulated by automatic pressure; control of the valve on the high ressurefeed pump 54. A second baille plate 1 is supported by the walls ofthe autoclave at an angle with the horizontal'to deflect the stream of emulsion y flowing over the vertical baiie plate 6 1, and to force it to take a downwardcourse below the supernatant aqueous solution of phenols. There is no' direct application of heat or other agency to promote circulation of the charge-'in section 65, and a quiet settling zone is thus maintained therein, where the the bottom of chamber 65, while the lighter insoluble residual oil rises to the top. .The liquid charge inthis section of the autoclave is therefore composed of three'distinct layers, namely, an upper la er ofoil/,an intermediate layer of emulsi ed'oilY and aqueous solution, and a bottom layer of the aqueous solution of phenols. The sectional elevation taken through the axis of the autoclave as illustrated in Fig. 1 of the drawing shows 4that at the up er end :of chamber 65 adjacent to the ba e plates 61 and 71 the single li u-id phase, e. g., the emulsion, has a depth su stantially equivalent to thetotal depth of the charge at that point. However, it will be noticed that as the emulsion advances ber of the preheater.

toward the outlet pipes at the lower end of chamber 65 its depth or thickness rapidly decreases because of its separation into' oil and aqueous components, so that its longitudinal section assumes roughly the shape of a V lying on its side. with the apex on the plane of demarcation between the oil and aqueous layers. The apex of the l will shift to the right whenever the rate of separation of emulsion into its aqueous and insoluble oil components increases. Conversely, the slower this rate of separation the greater will be the thickness of this layer of emulsion at the lower end of chamber 65 adjacent to the discharge pipes. In Fig. l a curved dotted line has been drawn to indicate what is thought to approximate the curve in which the interface between the emulsion and the upper layer will form. This interface will flatten out asit. approaches the point at which the'separation of the emulsion into oil and. aqueous components is completed, and from that. point to the discharge end of the a'utoclave the plane of demarcation 1 between the oil and aqueous components will of course be represented by a straight zontal line.

The insoluble residual or spent oil is removed 'lrom chamber 65 through a discharge pipe 72, e uipped with a valve 74, and is conducted y this pipe to coil 44 of preheater 40, through which it -ows in heat interchan ing relationship with liquids passing to the autoclave through the outer cham- From the preheater thepcooled oil is Withdrawn` into a tank 7 5 and is thence conducted to storage.' The aqueous solution of phenols is removed from chamber separately from the insoluble residual oil through a pipe 76, equipped -with a valve 78. It is conducted through coil 48 ofthe preheater 46 and is thus cooled by heat interchange' with the feed mixture of water and phenol-bearing oil passino' to the horiautoclave. `The solution is then exhausted into one of two separating tanks 80 and 82, Where it is further cooled if necessary. The phenols which are dissolved by water at the igh temperature prevailing in the autoclave are relatively insoluble in water at the low temperature 'which is maintained in the separating tank, and accordingly the phenols and the extraction water rapidly separate into layers. The phenol-saturated extraction water is run ofi into tank 84 and from there it can be passed through pipe 16 into the agitator 14 to be recirculated through the system in admixture with fresh oil. The crude phenols are drawn ofi' from tanks 80 andl'82 to a tank 86 vand are passed trom this tank to storage through a .pipe 88. The tanks 80 and 82 can be provided with cooling coils if additional cooling is necessary, and the charging and discharging pipes are equipped with valves so that both tanks can be used alternately. These tanks are of sufiicient capacity so that while one is being illed the layers of phenol and phenol-setmrated Water have sufficient time to separate 'out in the other tank and be drawn ot into their respective storage lines.

It will be apparent that the chief apparatus feature, of the invention, namely the divided and inclined cylindrical autoclave and the appurtenant charging and discharging equipment, can be used with a great number of combinations of auxiliary apparatus. This auxiliary apparatus may be widely different in construction, design. and arrangement from that described in the foregoing discussion and illustrated /in the drawings without departing materially 'from the broad principle of the invention. Each class of extraction processes has its own particular features and auxiliary apparatus requirements, and while the above description has been of necessity limited to one speciic arrangement, such as is'preferred for phenol extraction when water is used as the extraction agent, it is not intended by such des scription to limit the scope of the invention specifically to that one arrangement kof apparatus, even so far as apparatus for phenol recovery is concerned.

It has already been stated that the chief purpose of the inventionis to provide apparatus which is suitable for a process of continuous extraction under pressure. The control of the apparatus presents no roblems of particular diiiiculty. The fee to the high pressure pum and is determined y the static head in the 'tank 26. This head is maintained by the circulating pump 22, which is operated so that there is alwa s a slight overfiow into the agitator 14. e pressure in the autoclave 65 isdetermined both by the temperature of the charge 'and the rate of charging. The temperature 1s preferably maintained constant by thermostatic control of the 4fuel' valve 69, and the rate of charging is controlled b the steam valve on the high pressure fee pump 54, which in turn may be governed in accordance with the pressure in the autoclave. Further pressure regulation ,is possible by hand manipulation ot valves -74 and 7 8 on the discharge line.

The autoclave itself need not conform exactly to the design shown in the drawings, but regardless of type it is preferably supp'flrted at a slight angle from the horizontal.

e chief objects of this inclination are (l) To provide a vapor space that is located entirely over the hot mixing chamber, and only partially over the settling chamber of the same vessel.

(2) To provide a greater depth of layers in the settling chamber so that the products 54 is always constant' iaaoaa of extraction can be removed without danger of their becoming mixed with each other or with the emulsion.

The safety valve 68 is set to blow at a. pressure corresponding to a temperature somewhat higher than that at which the ex- A traction is conducted. When extracting phenols b water from the middle oil fractions of coa tar, it hasbeen found that the best compromise between the yield and purity ofl t e product is obtained at temperatures ranging from 200 to 225 C., and under pressures ranging between 15 and 25 atmospheres. Under these conditions the total time required for the extraction and subsequent gravity separation of the emulsion into its component layers of aqueous solution of phenols and of insoluble residual oils is usually less than five minutes.

' The preferred form of the invention having been thus described, what is claimed asl 1. An extraction apparatus comprising a vessel closed for o eration at super-atmospheric pressurean having its interior divided into a mixing chamber and a settling chamber, means forv introducing raw material to be extracted and a solvent into the mixing chamber and for agitating it, means for maintaining the charge in the vessel at mixing chamber, said means being arranged.

to agitate the charge therein, means for maintaining` the charge in the autoclave at an elevated temperature, and means for removing solution of extracted material from the settling chamber separately from insoluble residue.l a

3. lAn extraction apparatus comprising an autoclave, a baille plate dividing the interior of the autoclave into a mixing chamber and a settling chamber and arranged to maintain the charge in the settling chamber vin a quiescent state, lsaid baffle plate having its top spacedfrom the roof of the autoclave to permit emulsion of'extracted liquid and solvent to flow from the mixing chamber into the settling chamber,'mean"s for introducing liquid to be extracted and a solvent into the mixing chamber, said means being arranged to agitata the charge therein, means for heating the charge, means for maintaining the charge in the autoclave at an elevated temperature and pressure, and means for separately removing the soluble and the insoluble components of the liquid to be extracted from the settling chamber.

4. An extraction apparatus comprising an autoclave, means dividing the interior of the autoclave into a. mixing chamber and a settling chamber, said means being arranged to permit material toflow from the mixing chamber to the settling chamber, a charging nozzle arranged to introduce liquid to be extracted and a solvent into the mixing chamber `and to agitate the charge therein, means for 'heating the charge, means for maintaining the charge in the autoclave at an elevated temperature and pressure, and l means for separately removing the soluble .and insoluble components' of the liquid to be extracted from the settling chamber.

5'. 4An extraction apparatus comprising an autoclave closed for operation at super-atmospheric-pressure, a bame plate dividing the interior of the autoclave into a mixing chamber and a. settling chamber with a vapor space overlying and common to both ehambers, means for continuously introducing liquid to be extracted and a' solvent into the mixing chamber, means for continuously and separately removing the soluble and insoluble components of the liquid to be extracted from the settling chamber, and means for maintainingthe charge at the desired temperature and pressure.

6. An extraction apparatus comprising an autoclave closed for operation at super-atsis mospheric pressure, means for continuously introducing a charge of liquid to be. .exi tracted and a solvent into the autoclave, and

for agitating the charge in one part of vthe autoclave, means for maintaining the charge in the autoclave at an elevated temperature v and pressure, and discharge pipes verticallyspaced from each other and arranged to remove the solubleand insoluble components of the liquid to be extracted continuously and separately from the autoclave.

7. An extraction apparatus comprising a cylindrical autoclavev supported with its axis 'at an angle to the horizontal, means dividing 4the interior of the autoclave into an upper or mixing chamberA and a lower or lsettling chamber, charging means for introducing liquid to be extracted and a solvent into the upper or mixing chamber of,

the* autoclave and for agitating the charge therein, means for heating the charge, means for maintaining elevated temperatures and pressures within the autoclave, and means for separately removing the soluble and insoluble components of the liquid to be ex- 'f tracted from they lower or settlingl chamber of the autoclave.

8. An extraction apparatus com rising an autoclave having its interior divi ed into a mixing chamber and a settling chamber, means for continuously introducing liquid to be extracted anda solvent into the mixing chamber, means for maintaining the charge in the autoclave at an elevated temperature and pressure, means for continuously and separately removing the soluble and insoluble components of the liquid to be extracted 7 from the settling Ichamber, means for cooling the solution of the soluble components, and a settling tank having an inlet for the mixture of solvent and extract precipitated by the cooling of the solution and a valved outlet for removing the layers of solvent and extract separatedl by gravity separately therefrom.

9. An extraction apparatus comprising an autoclave having its interior divided into a mixing chamber and a settling chamber, a preheater having heating and cooling compartments, means for continuously passing a charge of liquid to be extracted and a solvent from the heating compartments of the preheater into the mixing chamber, and for agitating the charge in the mixing chamber. means for maintaining the charge 1n .the autoclave at an elevated temperature and pressure, and means for continuously passing hot solution ofsoluble components of the liquid to be extracted from the settling chamber through the cooling compartments of the preheater in heat interchanging relationship With the liquid passing through the heating compartments to the mixing chamber.

10. An extraction apparatus comprising an autoclave closed for operation at superatmospheric pressure and an agitator arranged to thorouvhly mix liquid to be extracted with fresli or previously saturated solvent, means for passing said mixture from the-agitator into the autoclave, means for agitatng the charge in one portion of the autoclave, means for maintaining simple seti tling of the charge into layers of solution of soluble and of insoluble components of the liquid in another portion of the autoclave, means for maintaining the charge at an elevated temperature and pressure, means for separately removin(y solution of soluble components and insoluble com'ponents from the autoclave, means for cooling `the solution of soluble components to separate the extract from the solvent, and means for returning the saturated solvent to the agitator.

1l. An extraction apparatus comprising Y an autoclave closed for operation at super- :ilmospheric pressure, means'for dividing the interior of the autoclave into a mixing chamber and a settling chamberhaving a common vapor space, mea-ns for introducing a cl'iarge of liquid to be extracted and a solvent into the mixing chamber and for agitating the charge in the mixing chamber, means for maintaining the charge at an into the mixing chamber, means for heating the charge, means for maintainin the charge in the autoclave at the desire temperature and pressure, means for continuously removin the soluble and insoluble components of t e liquid to be vextracted separately from the settling' chamber, means for controlling the rate at which the mixture is introduced into the autoclave, and other means for controlling the rate at which the soluble n and insoluble components are removed therefrom.

13. An extraction apparatus comprising an autoclave Adesigned for operation at superatmospheric pressure, means dividing the i11- terior of the'autoclave into a mixing chamber and a settling chamber, a charging nozzle arranged to discharge below the level of the charge in the mixin chamber, a number of discharge pipes lea ing from the settling chamber at different levels, a constant gravity feed tank and a charging pump with connections for continuously introduc-` ing liquid to be extracted and a'solvent into the mixin chamber, and means for continuously and separately removing soluble and insoluble components of the liquid to be extracted from the settling chamber through separate discharge pipes. y

14. An extraction apparatus comprising an autoclave, means for supporting the au toclave at an angle to the horizontal, means for heating the upper part of the autoclave, a charging nozzle arranged to introduce ma terial to be extracted into the upper enclosed part 4and a discharge pipe in the lower art of the autoclave for removing solution o extracted material therefrom, a preheater arranged to cool solution of extracted material removed from the autoclave by heat transfer With material to be extracted, a separating tank with a drawptl" pipe for Withdrawing separately the layers of extracted material and solvent components separated by gravity from the cool solution, and anV agitator for mixing solvent with fresh material to be extracted.

15. An extraction apparatus comprising an autoclave connected with an agitator, preh-eaters, separating tanks and pumping equipment, a furnace structure supporting the autoclave at an angle and arran ed for the combustion of fuel to furnish ieat to maintain the interior of the autoclave at a desired elevated'temperature, a pressure relief valve on the autoclave set to maintain a corresponding superatmospheric pressure therein, valves for regulating the rate of charging the autoclave with material to be extracted, valve for regulating'the rates at which solution of extracted material and insoluble residue are removed from the autoclave, and means dividing the charge in the autoclave into an extraction zone and a settling zone wherein solution of extracted Inaterial and insoluble residue' can separate into layers according Vto their relative specific gravities.

In testln'lony whereof I affix my signature ROLAND P. SOULE. 

